JP2916640B2 - Micro probe equipment - Google Patents

Description

Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for a micro probe used for measuring a coulometric value of a thickness of a metal coating.

[Prior Art] German Patent Application P 38 31 399.5 is known as a conventional device for this type of micro probe. Other similar devices are disclosed in U.S. Pat. No. 4,488,938 and German Patent 3046 198.

The German patent application P 38 31 399.5 discloses an outer sleeve which is generally provided with an outlet opening for the electrolyte solution and has a first connection for a pressure medium, an inner sleeve in this outer sleeve, A second space in the inner sleeve and opposite the outlet opening; a second connection for a pressure medium communicating with the second space; and a nozzle opening in the inner sleeve. A nozzle following the outlet opening in one space and leading from the second space to the outlet opening; and a connecting pipe connected at least to the second connecting part through a pressure medium, and the first space and the second space. at least indirectly with respect to space, at least one conductive and a pump causing working pressure P ₀ and P ₁ different in two of the low-pressure vibration (oszillierend) Micro Saguko equipment for measurement is disclosed.

In the micro-probe apparatus as described above, when the measurement state, that is, when the outlet opening is closed, the electrolyte solution is jetted once from the nozzle toward the measurement object depending on the position of the piston in the pump. Return to the first space. Alternatively, the electrolyte solution is injected from the first space to the outlet opening and toward the object to be measured, and is sucked again from the nozzle end. The frequency of this flow operation is about 1 Hertz.

[Problems to be Solved by the Invention] As is well known, the electrolyte solution as described above has erosive properties whether it is acidic or basic. As long as the normal operation as described above is performed, the electrolyte solution does not come out of the micro probe. However, despite being pointed out in an instruction manual or the like, the micro probe is often lifted during the measurement operation. Then, as a result, the electrolyte solution is ejected from the outlet opening at an extremely high speed. In this case, the electrolyte solution may be pushed out from both the first space and the second space.

The consequences or problems of such a phenomenon can easily be imagined. That is, the electrolyte solution is first lost. Further, there is a possibility that the coating layer is eroded over a wide range and becomes unusable. In addition, there is a problem that the electrolyte may jump into the operator's eyes, nose, mouth, etc., or may adhere to clothes and damage the fabric.

It is an object of the present invention to provide a micro probe device in which an electrolyte solution does not come out of an outlet opening even if it is erroneously lifted during a measurement operation.

[Means for Solving the Problems] An apparatus for a micro probe according to claim 1, which achieves the above object, comprises: (a) a valve device is provided between the pump and the probe; and a negative pressure P ₂ is overlapped at the operating state of the valve device, and the negative pressure is characterized by significantly lower than the maximum pressure in the working pressure P ₀ or P _1.

Pressure conditions as described above, for example as shown in claim 2, first the pump to produce a constant pressure to produce a minimum pressure P ₂ in the connecting pipe, associated to the connecting tube and the first space
A first circuit between the connection portion and the first circuit; a first valve in the first circuit; a second valve for the pressure medium in the first valve; and a region in which the pressure value of the medium is zero. And the second inlet can be periodically opened and closed.

 Preferably, the pressure medium is air.

Further, it preferred that the working pressure P ₀ and P ₁ is a negative pressure.

The second inlet of the first valve can be opened and closed by a needle valve.

It is preferable that a dustproof filter is provided before the needle valve.

A second circuit may be provided between the connection pipe and a second connection portion associated with the second space, the fluid resistance therebetween being smaller than that of the first circuit.

The outlet opening is preferably small enough to act capillaryly on the electrolyte solution.

It is preferable to provide an electrolyte liquid separator between the second space and the second circuit.

Several other features of the invention will be apparent from the detailed description of the invention that follows.

[Operation] According to the micro probe device according to the configuration of claim 1 described above, all the electrolyte solution is sucked back due to the large negative pressure corresponding to the amount of oscillation of the working pressures P ₀ and P ₁ ,
And it will not go out of the first space nor the second space. This should be compared to the pulsating DC current. That is, such a direct current causes a reciprocating phenomenon in the flow of electrons, and thus the same conditions as those of the case of the alternating current are generated. The DC voltage additionally applied to the true alternating current, which in this case corresponds to the first negative pressure, is however very high, so that a sufficient distance from the X-axis is maintained when describing this condition in rectangular coordinates. It is.

According to the second aspect of the present invention, the pump fundamentally generates a negative pressure, and the oscillating pressure can be generated only in the first circuit. For producing the negative pressure, for example, a mass production type pump in the field of diving equipment can be used.

According to the third aspect, the device can be operated under normal atmospheric conditions. At this time, the electrolyte solution does not oxidize therein.

 According to the fourth aspect, the working pressure is always a negative pressure.

According to the fifth aspect, the negative pressure can be very finely controlled.

According to claim 6, the function of the needle is not impaired.

With the configuration according to claim 7, the electrolyte solution is sucked back into the first space, and the separation of the electrolyte can be stopped only at this position and possibly in a subsequent circuit.

According to the eighth aspect, even when the pump is stopped, the electrolyte solution does not flow out of the micro probe.

With this configuration, the electrolyte liquid sucked back with a large kinetic energy never reaches the pump, and is possibly eliminated before a valve provided in the second circuit. . If the electrolyte solution is sucked out of the first space, a device for removing the electrolyte solution must be provided.

Example As shown in FIG. 1, a metal coating layer 2 to be measured is applied on a base material 1.

The micro probe 3 includes an outer sleeve 4 and an inner sleeve 6. These sleeves 4, 6 are substantially entirely made of plastic. The outer sleeve 4 has an outlet opening 7 formed on the lower side. The inner sleeve 6 transitions to the nozzle 8 on the lower side. The outer sleeve 4 and the inner sleeve 6 are hermetically and liquid-tightly sealed by a packing 9 shown schematically in FIG.
A first space 11 is provided between the outer sleeve 4 and the inner sleeve 6 or the nozzle 8. The nozzle 8
A second space 12 is provided in the inner sleeve 6 including Further, the outer sleeve 4 is provided with a first connection portion 13 on the upper end side of the first space 11, and the inner sleeve 6 is provided with a second connection portion 14 above the second space 12. I have.

The first circuit 16 extends from the first connection 13 to the branch position 17, and the second circuit 20 extends from the connection 14 to the branch position 17. From the branch position 17, a circuit 18 extends to another branch position 19. From this branch position 19, a circuit 21 and a circuit 22 are branched. The first circuit 16 has a valve 29 and the second circuit 20
Are provided with valves 31 respectively. Meanwhile, circuit 21
Is provided with a valve 23, and the circuit 22 is provided with a valve 24. The circuit 21 is connected to the suction nozzle 26 of the pump 28,
On the other hand, the circuit 22 is also connected to the pressure side nozzles 27 of the pump 28, respectively.

The valve 23 allows a connection from the mouth K connected to the suction nozzle 26 to the mouth G connected to the branch position 19, so that in this state the suction nozzle 26 is connected to the circuit 21. , Through the circuit 18, the branch position of the valves 29, 31
The 17 side communicates with the circuits 16 and 20. The nozzle H communicating with the outside air at the valve 23 can also be connected to the entrance G,
Is switched from the port K to the nozzle H, the outside air pressure is maintained in the circuits 21 and 18 and the circuits 16 and 20 on the branch position 17 side.

Similarly, the valve 24 can switch between the connection from the port P to the port L and the connection from the nozzle O to the port L.

Similarly, the valve 31 can switch between the connection from the port F to the port D and the connection from the port F to the nozzle E (external pressure).

The connection by the valves 23, 24, 31 is an open-close connection.

However, the valve 29 provided in the first circuit 16 has a needle valve structure, and a dustproof air filter 32 is provided in front of the nozzle A. In this valve 29, the tip of the needle can close the needle seat more or less by a method known per se. In this way, it is possible to adjust the pressure P ₁ shown in FIG. 3 finely. Needle valve 29 allows for a more or less flowable long-term ventilation. That is, a connection is established between the nozzle A and the port C. Next pressure P ₀ the pressure P ₁ is when allowed interrupted the connection extreme cases, i.e. low vibration operation will not occur.

Conversely, between the nozzles A and mouth C penetrates when the needle valve 29 is fully opened with the stroke motion of the needle, the pressure P ₁ in this case becomes a slight negative pressure, t axis in Figure 3 It will be located nearby. Since the optimum value exists at any position between the two, the liquid level 33 in the first space 11 and the liquid level 34 in the nozzle 8
Always swings with an amplitude X, for example, and the first space 11
And the second space 12 are never completely emptied or filled. This is because, if such a case occurs, air will reach the outlet opening 7 instead of the electrolyte solution. The amplitude X becomes larger or smaller depending on the degree of closing of the needle of the valve 29.

 The operation principle will be described below.

Filling the second space 12 with the electrolyte solution: The lower end of the micro probe 3 is immersed in the electrolyte solution storage tank. Pump sucks. Valve 29 is at port C-Nozzle A, while valve 31 is at port F-Port D. Therefore, the electrolyte solution is sucked from the storage tank into the second space 12 through the outlet opening 7.

Filling the first space 11 and the second space 12 of the micro probe 3 to the same level: the valve 31 is in the position of the port F-port D, the valve 29 is in the position of the port C-port B, and in this state the pump is 28 sucks. Therefore, the electrolyte solution maintains the liquid level 33, 34 at the same level.

Measurement: Valve 29 is alternately switched between mouth C-nozzle A position and mouth C-mouth B position. The valve 31 is located at the port F-port D, and the pump 28 sucks in this state.

Normal termination: The switching operation of the valve 29 is stopped. That is, mouth C-mouth B
To the position. The valve 31 is located at the nozzle E-port D. As a result, the electrolyte flows into the second space 12.

Next, when the valve 29 is switched to the position of the mouth C-nozzle A for a short time, the negative pressure in the first space 11 is reduced, whereby the electrolyte flows into the second space 12.

When the micro probe is mistakenly lifted during measurement: The pump 28 rotates, and the valve 29 is positioned between the port C and the port B and the port C.
-It is alternately switched between the nozzle A position. Atmospheric pressure is applied to the outlet opening 7. The amount of air flowing out of the first connection 13 is smaller than the amount flowing out of the second connection 14 because of the high fluid resistance which tends to suppress the flow. Thus, the electrolyte solution in the second space 12 is sucked upward, but the opening 43 of the nozzle 8 is slightly above the outlet opening 7 and the electrolyte flowing downward from the first space passes through the opening 43. Since it must pass, the electrolyte solution in the first space is likewise drawn upward.

Discharge of electrolyte solution: valve 29 at port C-nozzle A, valve 23 at nozzle H-port K, valve 31 at port F-port D, and still valve 24 at port L-port P The pump 28 is operated. As a result, the electrolyte flows out of the second space 12. still,
During normal operation, the valve 24 is, of course, at the mouth P-nozzle O position.

Cleaning of the second space 12: Same operation as filling and discharging of the electrolyte solution.

Although the above-described micro probe device has various types of operation methods as described above, the function when the micro probe 3 is inadvertently lifted is particularly useful.

FIG. 4 is an exploded side view showing a specific example of the micro probe 3, and FIG. 4 shows an outer sleeve 4, an inner sleeve 6 having a nozzle 8, a packing 9, a connecting portion 14, a second space 12,
The outlet opening 7 and the circuit 20 are shown.

An electrode 42 is fixed to the outer sleeve 4 in a penetrating state. This electrode 42 corresponds to the electrode 33 of DE 30 46 198. When this outer sleeve 4 is fixed to the inner sleeve 6, the opening 43 of the nozzle 8 is located concentrically to the left of the outlet opening 7 of the outer sleeve 4, and the left terminal rim located before this outlet opening 7. 44 is the color 48 of the inner sleeve 6
Seated air-tight and liquid-tight on the
, The left end surface 47 is an annular surface of the inner sleeve 6.
Cover 46.

The micro probe 3 has a substantially rotationally symmetric design with respect to the geometrical long axis 49. The inner sleeve 6 transitions on the left-hand side in FIG. 4 to an enlarged part 51, which is also rotationally symmetric. A relatively large leftward opening cup 52 is formed in the enlarged portion 51,
The cup 52 communicates with the second space 12. The bottom of the cup 52 is concave, so that with the micro-probe 3 in a vertical position, the electrolyte which sometimes reaches this cup 52 can be transferred to the second space 12 quickly and without residue. Has become.

A ring flange 54 is provided on the left side of the enlarged portion 51, and an O-ring 56 is fitted on the outer peripheral surface thereof. The ring flange 54 can be hermetically inserted inside the outer peripheral flange 57 of the intermediate piece 58.

The intermediate piece 58 forms an electrolyte liquid separator together with the cup 52, and has a separate screw-in cartridge 59.
It has.

A ring head 61 is formed on the cartridge 59, and the outer diameter of the ring head 61 is smaller than the inner diameter of the cup 52. The ring head 61 is also formed with a concave recess 62 that opens to the right, and the recess 62 forms a sharp edge 63 at the right end. Cartridge 59
On the left side, a short screw shank 64 having a diameter much smaller than the ring head 61 is formed.
An external screw 66 is screwed into the screw shank 64. However, since the external screw 66 is screwed only up to a broken line 67 excluding the root of the screw shank 64, the screw shank 64 cannot be completely screwed. Two grooves 68 are machined in opposing positions on the diameter of the screw shank 64 over its entire length. These grooves 68
4 extends from left to right in FIG. 4 and further penetrates to the right of the broken line 67.

In the intermediate piece 58, the left side of the outer peripheral flange 57 is shifted to a bottom 69, and a screw hole is coaxially formed in the bottom 69.
71 has been processed. The outer screw 66 of the screw shank 64 can be screwed into the screw hole 71 up to a broken line 67. A cup 72 serving as a third space is formed on the left side of the bottom 69, and the left side thereof is connected to a ring flange 73. This ring flange 73 can be inserted from outside.
A ring 74, and these dimensions are exactly the same as the ring flange 54 and the O-ring 56; Therefore, when the intermediate piece 58 is not used, the cover 76 can be directly and airtightly seated on the enlarged portion 51.

The cover 76 has an outer peripheral flange 77. The outer peripheral flange 77 is air-tight and liquid-tight.
Fits. The cover 76 has a through hole 78 at the center, and the through hole 78 opens to the connection portion 14. 4th
According to the figure, this connecting part 14 has the shape of a nipple.

The micro probe normally formed as described above is a U.S. patent
4 held vertically or almost vertically as shown in FIG. 1 of 488.938.

Now, in order to lifted by mistake during measuring micro Saguko 3 as described above, when the outlet opening 7 is separated from the measurement surface, an electrolyte solution for the opening 43 is strong negative pressure P ₂ of the inner sleeve second Suction into space 12. Due to the large kinetic energy of this suction, the electrolyte cannot be kept stationary in the second space 12 and rises to the cup 52. Since the diameter of the cup 52 is larger than that of the second space 12, the cup 52 once expands, so that a part of the kinetic energy of the electrolyte solution disappears. Nevertheless, any liquid still striking into the recess 62 will thereby turn downward. The downward liquid brakes the rising liquid. Therefore, the electrolyte solution temporarily stops in the cup 52 and returns to the second space 12 again. By the way, ring head 61
The groove 68 will be in the blind spot of the electrolyte liquid jet. Therefore, the electrolyte does not enter the circuit 20, despite the large negative pressure from the circuit 20 reaching the cup 52 via the groove 68 and the outside of the ring head 61. The sharp edge 63 of the ring head 61 forms an edge for reversing the traveling direction of the electrolyte solution.

By the way, when the micro probe 3 is erroneously lifted, the electrolyte solution moves upward with a large energy as described above. Therefore, in some cases, the micro probe 3 having the structure as shown in FIG. May be. In such a case, the circuit on the left side of the valve 31
A separator container 36 as shown in FIG. The container body 37 of the separator container 36 is plugged on the upper side.
Closed by 38. An upright pipe 39 is provided through the stopper 38 in a gastight manner. This pipe 39 forms one end of the circuit 20 which is continuous with the connection part 14, and the container body
It opens at some distance from the bottom of 37. on the other hand,
The container body 37 has a through hole 41 formed at a position sufficiently higher than the opening of the rising pipe 39, and the circuit 20 on the valve 31 side is hermetically inserted into the through hole 41.
When such a separator container 36 is provided, the electrolyte solution accumulates below the container main body 37 even if it enters the circuit 20 across the connection portion 14. Electrolyte solution 40 collected under this container body 37
Because the opening of the rising pipe 39 is at a large distance from the through hole 41, the through hole
It does not enter the circuit 20 on the valve 31 side inserted in 41.

[Effects of the Invention] According to the first aspect, even if the microscrew is accidentally lifted during the measurement operation, the electrolyte does not jump out, so that the electrolyte is not lost from the probe. Further, there is no danger that the coating layer will be eroded and become unusable. Further, the operator does not jump into the eyes, nose, mouth, etc., and does not hurt the cloth by clothes or the like.

According to the second aspect, a specific configuration for obtaining the vibration pressure is obtained.

According to claim 3, a practical device can be provided.

According to claim 4, the electrolyte solution is sucked back under any pressure.

 According to the fifth aspect, an optimal negative pressure can be obtained.

According to claim 6, the operating condition is correctly maintained for a long time.

According to the seventh aspect, the separation position of the electrolyte solution can be specified.

According to claim 8, even when the pump is stopped, no damage is caused by the outflowing electrolyte solution.

According to claim 9, the pump is not damaged by the electrolyte solution.

[Brief description of the drawings]

FIG. 1 is a schematic diagram of a circuit, FIG. 2 is a cross-sectional view of a separator container, FIG. 3 is a graph showing pressure in a first space, and FIG.
The figure is an exploded side view of the micro probe. 4 ... outer sleeve, 6 ... inner sleeve 11 ... first space, 12 ... second space 13 ... first connection part, 14 ... second connection part 28 ... pump 29,31,23,24 …… Valve devices P ₀ , P ₁ …… Working pressure, P ₂ …… Negative pressure

──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. ⁶ , DB name) G01N 27/42

Claims (20)

(57) [Claims] 1. An outer sleeve having an outlet opening for an electrolyte solution at one end and having a first connection for a pressure medium, an inner sleeve in the outer sleeve, and a first sleeve between the outer sleeve and the inner sleeve. A second space in the inner sleeve and opposite the outlet opening; a second connection for a pressure medium communicating with the second space; and a nozzle opening in the first space. A nozzle connected to the outlet opening from the second space, the connection tube being connected to at least the second connection portion through a pressure medium, and the first space and the second space being connected to each other.
At least indirectly with respect to space, at least one pump for generating two different working pressures P ₀ and P ₁ oscillating at low pressure and a microprobe apparatus for coulometric measurement of the thickness of a metal coating, , (a) a valve device is provided between the pump and Saguko, (b) at least one working pressure using the pressure P ₀ or the maximum pressure from the well of P ₁ at the operating conditions of the pump and valve device apparatus for micro Saguko, characterized in that overlaps with low negative pressure P _2. 2. A pump produces a constant pressure to produce a minimum pressure P ₂ in the connection pipe, the first circuit is provided between the first connection part associated with the connecting tube and the first space, the first circuit Is provided with a first valve, and the first valve has a second inlet for the pressure medium, and the pressure value of the medium has a region of zero, and the second inlet periodically opens and closes. 2. The device for a micro probe according to claim 1, wherein the device can be used. 3. The device according to claim 1, wherein the pressure medium is air. 4. The device according to claim 1, wherein the working pressures P ₀ and P ₁ are negative pressures. 5. The micro probe device according to claim 2, wherein the second inlet of the first valve can be opened and closed by a needle valve. 6. The device according to claim 5, wherein a dust filter is provided in front of the needle valve. 7. A second circuit is provided between a second connection part and a connection pipe associated with the second space, and a fluid resistance between the second connection part and the connection pipe is higher than that of the first circuit. 2. The device for a micro probe according to claim 1, wherein the size of the micro probe is also small. 8. The microprobe apparatus according to claim 1, wherein the outlet opening is small and acts capillaryly on the electrolyte solution. 9. The micro probe device according to claim 7, wherein an electrolyte liquid separator is provided between the second space and the second circuit. 10. A separator having a reflector for electrolyte solution sucked back over the extension of the nozzle, and at least outside the extension line of the nozzle end and outside the reflector for repelling the electrolyte solution, communicating with the second connection portion. The device for a micro probe according to claim 9, wherein a through hole for one pressure medium is provided. 11. The device according to claim 10, wherein the reflection plate has a concave shape toward the nozzle. 12. The device according to claim 11, wherein the reflector has a sharp edge facing the nozzle. 13. The micro probe according to claim 10, wherein the reflector is provided coaxially at a peripheral portion with respect to the second space at a distance. Equipment. 14. The micro probe device according to claim 10, wherein a third space having a through hole formed therein is provided behind the second space. 15. The device according to claim 14, wherein the through-hole opens at the lowermost end of the third space when the probe is held vertically. 16. The reflector according to claim 10, wherein the back surface of the reflector is spaced from the cover of the second space, and the through hole starts at the back surface of the reflector. Micro probe device. 17. The method according to claim 17, wherein the reflector is inserted into the hole of the cover in the second space with one projection.
17. The device for a micro probe according to any one of 10 to 16. 18. The micro-probe apparatus according to claim 10, wherein the through-hole is provided around the hole and / or the projection. 19. The device according to claim 10, wherein the second space is shifted to the enlarged portion by a reflection plate. 20. The device according to claim 9, wherein the separator is a container separator, which is provided in front of a valve in the second circuit.